1、Manual of PetroleumMeasurement StandardsChapter 10Sediment and WaterSection 8Standard Test Method for Sediment in Crude Oil by Membrane FiltrationSECOND EDITION, NOVEMBER 2005REAFFIRMED, MARCH 2010Manual of PetroleumMeasurement StandardsChapter 10Sediment and WaterSection 8Standard Test Method for S
2、ediment in Crude Oil by Membrane FiltrationMeasurement CoordinationSECOND EDITION, NOVEMBER 2005REAFFIRMED, MARCH 2010SPECIAL NOTES API publications necessarily address problems of a general nature. With respect to particular circumstances, local, state, and federal laws and regulations should be re
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16、ndards and Publications Department, API, 1220 L Street, NW, Washington, DC 20005, standardsapi.org. iii CONTENTS Page 1. SCOPE . 1 2. REFERENCED DOCUMENTS 1 2.1 ASTM Standards 1 2.2 API Standards. 1 2.3 ISO Standard 1 3. SUMMARY OF TEST METHOD. 1 4. SIGNIFICANCE AND USE 1 5. APPARATUS. 2 6. REAGENTS
17、 . 2 7. SAMPLING, TEST SPECIMENS . 2 8. PROCEDURE 3 9. CALCULATION 3 10. REPORT. 3 11. PRECISION AND BIAS 4 12. KEYWORDS . 4 ANNEX A1. SAFETY PRECAUSTIONS TO AVOID STATIC DISCHARGE 4 SUMMARY OF CHANGES 5 Figure 1 Membrane Filtration Assembly 2 Table 1 Precision Intervals 4 Designation: D 4807 05e1De
18、signation: Manual of Petroleum Measurement Standards (MPMS), Chapter 10.8An American National StandardStandard Test Method forSediment in Crude Oil by Membrane Filtration1This standard is issued under the fixed designation D 4807; the number immediately following the designation indicates the year o
19、foriginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department
20、 of Defense.e1NOTEFootnote 5 was updated editorially in August 2005.1. Scope*1.1 This test method covers the determination of sedimentin crude oils by membrane filtration. This test method has beenvalidated for crude oils with sediments up to approximately0.15 mass %.1.2 The accepted unit of measure
21、 for this test method ismass %, but an equation to convert to volume % is provided(see Note 6).1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafety concerns, if any,
22、 associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see 6.1 and Annex A1.2. Referenced Documents2.1 ASTM Standards
23、:2D 473 Test Method for Sediment in Crude Oils and FuelOils by the Extraction Method (API MPMS Chapter 10.1)D 4057 Practice for Manual Sampling of Petroleum andPetroleum Products (API MPMS Chapter 8.1)D 4177 Practice for Automatic Sampling of Petroleum andPetroleum Products (API MPMS Chapter 8.2)D 4
24、865 Guide for Generation and Dissipation of StaticElectricity in Petroleum Fuel SystemsD 5854 Practice for Mixing and Handling of LiquidSamples of Petroleum and Petroleum Products (APIMPMS Chapter 8.3)2.2 API Standards:3MPMS Chapter 8.1 Manual Sampling of Petroleum andPetroleum Products (ASTM Practi
25、ce D 4057)MPMS Chapter 8.2 Automatic Sampling of Petroleum andPetroleum Products (ASTM Practice D 4177)MPMS Chapter 8.3 Mixing and Handling of Liquid Samplesof Petroleum and Petroleum Products (ASTM PracticeD 5854)MPMS Chapter 10.1 Test Method for Sediment in CrudeOils and Fuel Oils by the Extractio
26、n Method (ASTM TestMethod D 473)2.3 ISO Standard:4ISO 5272:1979 Toluene for Industrial UseSpecifications3. Summary of Test Method3.1 A portion of a representative crude oil sample isdissolved in hot toluene and filtered under vacuum through a0.45-m porosity membrane filter. The filter with residue i
27、swashed, dried, and weighed to give the final result.4. Significance and Use4.1 A knowledge of the sediment content of crude oil isimportant both in refinery operations and in crude oil com-merce.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants an
28、d the API Committee on Petroleum Measure-ment, and is the direct responsibility of Subcommittee D02.02/COMQ, the jointASTM-API committee on Static Petroleum Measurement.This test method has beenapproved by the sponsoring committee and accepted by the Cooperating Societiesin accordance with establish
29、ed procedures.Current edition approved June 1, 2005. Published September 2005. Originallyapproved in 1988. Last previous edition approved in 1999 as D 480788(1999).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Boo
30、k of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Published as Manual of Petroleum Measurement Standards.Available from theAmerican Petroleum Institute (API), 1220 L St., NW, Washington DC 20005.4Available from American National Standards Institu
31、te (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.1*A Summary of Changes section appears at the end of this standard.5. Apparatus5.1 Funnel and Filter Support AssemblyUse an assemblydesigned to hold 47-mm diameter filters as was used in thedevelopment of this test method (see Fig. 1).55.1.1 Fi
32、lter FunnelUse a filter funnel with a 250 mLminimum capacity. The lower part of the funnel has a 40-mminside diameter and is designed to secure the 47-mm diameterfilter against the filter support. The funnel can be jacketed tofacilitate heating the solvent funnel and sample during filtering.NOTE 1Us
33、e of a glass funnel should minimize the effect of staticelectricity when filtering.5.1.2 Filter SupportUse a support base for the filter thathas a porous scintered glass center section about 40 to 43 mmin diameter. The support base is designed to fit securely againstthe funnel holding the filter in
34、place over the porous section.The filter supports stem should be long enough to extend downinto the filter flask such that the end is below the vacuumconnection.5.1.3 Clamp AssemblyUse a spring or screw type clampto secure the funnel to the filter support. The clamp should betight enough to prevent
35、the solvent from leaking through at thejunction between the glass and filter membrane. The exteriordimensions of the funnel and support are designed to facilitateclamping the two pieces together.5.1.4 Rubber StopperUse a single-hole, capable of hold-ing the lower stem of the filter support securely
36、onto thefiltering flask.5.1.5 Vacuum Filtering FlaskUse a 500 mL or largervacuum filtering flask.5.2 Membrane FilterUse a nylon membrane filter, 47 mmin diameter with 0.45-m pore size.65.3 OvenUse an oven capable of maintaining a tempera-ture of 105 6 2C (220 6 4F).5.4 Vacuum PumpUse a vacuum pump c
37、apable of reduc-ing and maintaining the pressure at 80 kPa (24 in. Hg)during the filtering.5.5 Analytical BalanceUse an analytical balance capableof measuring to the nearest 0.0001 g. Verify the balance, atleast annually, against weights traceable to a national metrol-ogy institute such as the Natio
38、nal Institute of Standards andTechnology (NIST).5.6 Heating Coil for Filter AssemblyUse copper tubing(3.175 mm or18-in. diameter) wound around the funnel on thefilter apparatus and connected to a circulating bath to maintainthe oil in the funnel at 90 6 2C (see Fig. 1). Alternativemethods of heating
39、 the funnel such as heating tape or glassthermal jacket could also be used.5.7 MixerUse a nonaerating, high-speed mixer meetingthe verification efficiency requirements specified in PracticeD 5854 (API MPMS Chapter 8.3). Either insertion mixers orcirculating mixers are acceptable provided they meet t
40、hecriteria in Practice D 5854 (API MPMS Chapter 8.3).5.8 Cooling VesselUse a desiccator or other type oftightly covered vessel for cooling the membrane filter beforeweighing. The use of a desiccant/drying agent is not recom-mended.5.9 Ground/Bond WireUse a 0.9122.59 mm (No. 10through No. 19) bare st
41、randed flexible, stainless steel or copperwire installed in the flask through the vacuum connection andconnected to ground.6. Reagents6.1 TolueneReagent grade chemicals shall be used in alltests. Unless otherwise indicated, it is intended that all reagentsshall conform to the specifications of the C
42、ommittee onAnalytical Reagents of the American Chemical Society, wheresuch specifications are available,7or to Grade 2 of ISO 5272.Other grades may be used, provided it is first ascertained thatthe reagents lot or batch is of sufficiently high purity to permitits use without lessening the accuracy o
43、f the determination.(WarningFlammable. Keep away from heat, sparks andopen flame. Vapor harmful. Toluene is toxic. Particular careshall be taken to avoid breathing the vapors and to protect theeyes. Keep the container closed. Use with adequate ventilation.Avoid prolonged or repeated contact with the
44、 skin.)7. Sampling, Test Specimens7.1 Sampling, shall include all the steps required to obtain arepresentative portion of the contents of any pipe, tank, or othersystem, and to transfer the sample into the laboratory testcontainer. The laboratory test container and sample volumeshall be of sufficien
45、t dimensions and volume to allow mixing asdescribed in 7.3.1. Mixing is required to properly dispersesediment as well as any water present in the sample.7.2 Laboratory SampleUse only representative samplesobtained as specified in Practice D 4057 (API MPMS Chapter8.1) or Practice D 4177 (API MPMS Cha
46、pter 8.2) for this testmethod. Analyze samples within two weeks after taking thesample. Retaining samples longer may affect the results.7.3 Sample PreparationThe following sample prepara-tion and handling procedure shall apply.7.3.1 Mix the test sample of crude oil at room temperaturein the original
47、 container immediately (within 15 min) before5The following filtration assembly was used in generating the precision:Millipore Corp., Ashly Rd., Bedford, MA 01730. Other filtration assemblies alsomay be acceptable.6The following filter was used in generating the precision: MSI Nylon 60Membrane Filte
48、r from Fisher Scientific, Catalog Number NO-4-SP047-00. Othernylon filters of 0.45-m porosity also may be acceptable.7Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical S
49、ociety, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.FIG. 1 Membrane Filtration AssemblyD480705e12analysis to ensure complete homogeneity. A test sample drawndirectly from a large volume dynamic mixing system shall beanalyzed within 15 min or else remix as follows:NOTE 2Analysis should follow mixing as soon as possible. The15-min interval mentioned above is a general guideline which may notapply to al
